SAMPLING METHODS AND METHODS OF ANALYSIS FOR THE OFFICIAL CONTROL OF THE LEVELS OF LEAD, CADMIUM, MERCURY

CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS

SUBSIDIARY LEGISLATION 437.66

SAMPLING METHODS AND METHODS

OF ANALYSIS FOR THE OFFICIAL CONTROL

OF THE LEVELS OF LEAD, CADMIUM, MERCURY

AND 3-MCPD IN FOODSTUFFS RULES

8th April, 2005

LEGAL NOTICE 98 of 2005.

(1) The title of these rules is the Sampling Methods and

Methods of Analysis for the Official Control of the Levels of Lead,

Cadmium, Mercury and 3-MCPD in Foodstuffs Rules.

(2) The scope of these rules is to implement the rules found

under European Union Council Directive 2001/22/EC on the

sampling methods and the methods of analysis for the official

control of the levels of lead, cadmium, mercury and 3-MCPD in

foodstuffs.

METHODS OF SAMPLING FOR OFFICAL CONTROL OF THE LEVELS OF

LEAD, CADMIUM, MERCURY AND 3-MCPD IN CERTAIN FOODSTUFFS

1. PURPOSE AND SCOPE

Samples intended for the official control of the levels of lead, cadmium, mercury

and 3-MCPD contents in foodstuffs shall be taken according to the methods

des c r i bed b e l ow. A gg re ga t e s a mp l e s t hus obtained shall be considered as

representative of the lots or sublots from which they are taken. Compliance with

maximum levels laid down in Regulation (EC) No 466/2001 shall be established on

the basis of the levels determined in the laboratory samples.

2. GENERAL PROVISIONS

2.1. Personnel

Sampling shall be performed by an authorised qualified person as specified by

Malta.

2.2. Material to be sampled

Each lot which is to be examined must be sampled separately.

2.3. Precautions to be taken

In the course of sampling and preparation of laboratory samples precautions must

be taken to avoid any changes which would affect the lead, cadmium, mercury and 3-

MCPD contents, adversely affect the analytical determination or make the aggregate

samples unrepresentative.

2.4. Incremental samples

As far as possible incremental samples shall be taken at various places distributed

throughout the lot or sublot. Departure from this procedure must be recorded in the

record provided for under 2.8.

2.5. Preparation of the aggregate sample

The aggregate sample is made up by uniting all incremental samples. It shall be at

least 1 kg unless not practical, e.g. when a single package has been sampled.

2.6. Subdivision of aggregate sample in laboratory samples for enforcement,

defence and referee purposes

The laboratory samples for enforcement, trade (defence) and referee purposes

shall be taken from the homogenised aggregate sample unless this conflicts with

Veterinary Services’ regulations on sampling. The size of the laboratory samples for

enforcement shall be sufficient to allow at least for duplicate analyses.

2.7. Packaging and transmission of aggregate and laboratory samples

Each aggregate and laboratory sample shall be placed in a clean, inert container

offering adequate protection from contamination, from loss of analytes by adsorption

to the internal wall of the container and against damage in transit. All necessary

precautions shall be taken to avoid change of composition of the aggregate and

laboratory samples which might arise during transportation or storage.

2.8. Sealing and labelling of aggregate and laboratory samples

Each sample taken for official use shall be sealed at the place of sampling and

identified following the Veterinary Services’ regulations. A record must be kept of

each sampling, permitting each lot to be identified unambiguously and giving the

CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS

date and place of sampling together with any additional information likely to be of

assistance to the analyst.

3. SAMPLING PLANS

Sampling should ideally take place at the point where the commodity enters the

food chain and a discrete lot becomes identifiable. The sampling method applied

shall ensure that the aggregate sample is representative for the lot that is to be

controlled.

3.1. Number of incremental samples

In the case of liquid products for which a homogeneous distribution of the

contaminant in question can be assumed within a given lot, it is sufficient to take one

incremental sample per lot which forms the aggregate sample. Reference to the lot

number shall be given. Liquid products containing hydrolysed vegetable protein

(HVP) or liquid soya sauce shall be shaken well, or homogenised by other suitable

means, before the incremental sample is taken.

For other products, the minimum number of incremental samples to be taken from

the lot shall be as given in Table 1. The incremental samples shall be of similar

weight. Departure from this procedure must be recorded in the record provided for

under 2.8.

Table 1: Minimum number of incremental samples to be taken from the lot

Weight of lot (kg)

Minimum number of incremental samples to be taken

< 50

50 to 500

> 500

If the lot consists of individual packages, then the number of packages which shall

be taken to form the aggregate sample is given in Table 2.

Table 2: Number of packages (incremental samples) which shall be taken to form

the aggregate sample if the lot consists of individual packages

Number of packages or units in the lot

Number of packages or units to be taken

1 to 25

1 package or unit

26 to 100

About 5%, at least 2 packages or units

> 100

About 5%, at maximum 10 packages or units

4. COMPLIANCE OF THE LOT OR SUBLOT WITH THE SPECIFICATION

The control laboratory shall analyse the laboratory sample for enforcement at least

in two independent analyses, and calculate the mean of the results. The lot is

accepted if the mean conforms to the respective maximum level as laid down in

Regulation (EC) No 466/2001. It is rejected if the mean exceeds the respective

maximum level.

CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS

For the purposes of these rules, and unless context

otherwise requires -

"aggregate sample" means the combined total of all the

incremental samples taken from the lot or sublot;

"the Commission" means the European Commission;

"the Community" means the European Community as established

under the Treaty establishing the European Community;

"the competent authority" means the Veterinary Services within

Malta as provided under article 2 of the Veterinary Services Act;

"incremental sample" means a quantity of material taken from a

single place in the lot or sublot;

"laboratory sample" means the sample intended for the

laboratory;

"lot" means an identifiable quantity of food delivered at one time

a n d d e t e r m i n e d b y th e v e t e r i n ary official to ha ve common

characteristics, such as origin, variety, type of packing, packer,

consignor or markings. In the case of fish, also the size of fish shall

be comparable;

"Member State" means a State which is a Member within the

European Community;

"sublot" means a designated part of a large lot in order to apply

the sampling method on that designated part. Each sublot must be

physically separated and identifiable;

"third country" means a State which is not a Member within the

European Community;

CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS

"Veterinary Services" means the competent authority within the

territory of Malta as established under article 2 of the Veterinary

Services Act.

SAMPLE PREPARATION AND CRITERIA FOR METHODS OF ANALYSIS

USED IN OFFICAL CONTROL OF THE LEVELS OF LEAD, CADMIUM,

MERCURY AND 3-MCPD IN CERTAIN FOODSTUFFS

1. INTRODUCTION

The basic requirement is to obtain a representative and homogeneous laboratory

sample without introducing secondary contamination.

2. SPECIFIC SAMPLE

PREPARATION

PROCEDURES

FOR

LEAD,

CADMIUM AND MERCURY

There are many satisfactory specific sample preparation procedures which may be

used for the products under consideration. Those described in the draft CEN

Standard ‘Foodstuffs - Determination of trace elements - Performance criteria and

general consideration’ have been found to be satisfactory (a) but others may be

equally valid.

The following points must be noted for any procedure used

-

bivalve molluscs, crustaceans and small fish: where these are normally

eaten whole, the viscera are to be included in the material to be

analysed,

-

vegetables: only the edible portion of is to be tested, with note to be

taken of the requirements of the Regulation (EC) No 466/2001.

3. METHOD OF ANALYSIS TO BE USED BY THE LABORATORY AND

LABORATORY CONTROL REQUIREMENTS

3.1. Definitions

A number of the most commonly used definitions that the laboratory will be

required to use are given below

r = repeatability, the value below which the absolute difference between two

single test results obtained under repeatability conditions (i.e., same sample, same

operator, same apparatus, same laboratory, and short interval of time) may be

expected to lie within a specific probability (typically 95%) and hence r = 2,8 × sr.

sr = standard deviation, calculated from results generated under repeatability

conditions.

RSDr = relative standard deviation, calculated from results generated under

repeatability conditions [(sr / x -) × 100], where x - is the average of results over all

laboratories and samples.

R = reproducibility, the value below which the absolute difference between single

test results obtained under reproducibility conditions (i.e., on identical material

obtained by operators in different laboratories, using the standardised test method),

may be expected to lie within a certain probability (typically 95%); R = 2,8 × sR.

sR = standard deviation, calculated from results under reproducibility conditions.

RSDR = relative standard deviation calculated from results generated under

reproducibility conditions [(sR / x-) x 100]

HORRATr = the observed RSDr divided by the RSDr value estimated from the

Horwitz equation using the assumption r = 0,66R

HORRATR = the observed RSDR value divided by the RSDR value calculated

from the Horwitz equation (b).

CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS

3.2. General requirements

Methods of analysis used for food control purposes must comply whenever

possible with the provisions of paragraphs 1 and 2 of the Annex to Directive 85/591/

EEC.

For the analysis of lead in wine, Commission Regulation (EEC) No 2676/90

determining Community methods for the analysis of wines lays down the method to

be used in Chapter 35 of its Annex.

3.3. Specific requirements

3.3.1. Lead, cadmium and mercury analyses

Specific methods for the determination of lead, cadmium and mercury contents are

not prescribed. Laboratories shall use a validated method that fulfils the performance

criteria indicated in Table 3. Where possible, the validation shall include a certified

reference material in the collaborative trial test materials.

Table 3: Performance criteria of methods for lead, cadmium and mercury analyses

Parameter

Value / comment

Applicability

Foods specified in Regulation (EC) No 466/2001

Detection limit

No more than one tenth of the value of the specification in

Regulation (EC) No 466/2001, except if the value of the

specification for lead is less than 0,1mg/kg. For the latter,

no more than one fifth of the value of the specification

Limit of quantification No more than one fifth of the value of the specification in

Regulation (EC) No 466/2001, except if the value of the

specification for lead is less than 0,1 mg`kg. For the latter,

no more than two fifths of the value of the specification

Precision

HORRATr or HORRATR values of less than 1,5 in the

validation collaborative trial

Recovery

80 - 120% (as indicated in the collaborative trial)

Specificity

Free from matrix or spectral interferences

3.3.2. 3-MCPD analysis

Specific methods for the determination of 3-MCPD contents are not prescribed.

Laboratories shall use a validated method that fulfils the performance criteria

indicated in Table 4. Where possible, the validation shall include a certified

reference material in the collaborative trial test materials. A specific method has

been validated by collaborative trial and has been shown to meet the requirements of

Table 4 (c).

Table 4: Performance criteria of methods for 3-MCPD analysis

Criterion

Recommended value

Concentration

Field blanks

Less than the detection limit

-

Recovery

75 - 110%

All

Limit of quantification

10 (or less) ìg/kg on a dry

-

matter basis

Standard deviation of the field

Less than 4 ìg/kg

-

blank signal

CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS

In-house precision estimates -

< 4 ìg/kg

20 ìg/kg

standard deviation of replicate

< 6 ìg/kg

30 ìg/g

m e a s u r e m e n t s a t d i ff e r e n t

< 7 ìg/kg

40 ìg/kg

concentrations

< 8 ìg/kg

50 ìg/kg

< 15 ìg/kg

100 ìg/kg

3.4. Estimation of the analytical trueness and recovery calculations

Wherever possible the trueness of the analysis shall be estimated by including

suitable certified reference materials in the analytical run.

The ‘Harmonised Guidelines for the Use of Recovery Information in Analytical

Measurement’ (d) developed under the auspices of IUPAC/ISO/AOAC shall be taken

into account.

The analytical result shall be reported corrected or uncorrected. The manner of

reporting and the level of recovery must be reported.

3.5. Laboratory quality standards

Laboratories must comply with Directive 93/99/EEC.

3.6. Expression of results

The results shall be expressed in the same units as the maximum levels laid down

in Regulation (EC) No 466/2001.

Malta shall take all measures necessary to ensure that the

sampling for the official controls of the levels of lead, cadium,

mercury and 3-MCPD in foodstuffs is carried out in accordance

with the methods described in Schedule I.

Malta shall take all measures necessary to ensure that

sample preparation and methods of analyses used for the official

control of the levels of lead, cadmium, mercury and 3- MCPD in

foodstuffs comply with the criteria described in Schedule II to

these rules.

When Malta adopts these provisions, the provisions shall

contain a reference to these rules or shall be accompanied by such

reference at the time of their official publication. The procedure for

such reference shall be that applicable in Malta.

CADMIUM, MERCURY AND 3-MCPD IN FOODSTUFFS